CN113186416A - SiC reinforced copper-based composite material and preparation method thereof - Google Patents
SiC reinforced copper-based composite material and preparation method thereof Download PDFInfo
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- 239000010949 copper Substances 0.000 title claims abstract description 137
- 239000002131 composite material Substances 0.000 title claims abstract description 94
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 59
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002245 particle Substances 0.000 claims abstract description 113
- 239000011521 glass Substances 0.000 claims abstract description 38
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 12
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 12
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 12
- 230000005496 eutectics Effects 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- -1 silicate ester Chemical class 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 4
- 230000007704 transition Effects 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000011156 metal matrix composite Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 45
- 238000005452 bending Methods 0.000 description 23
- 238000012360 testing method Methods 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 4
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 4
- 230000003014 reinforcing effect Effects 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007676 flexural strength test Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000005355 lead glass Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0005—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with at least one oxide and at least one of carbides, nitrides, borides or silicides as the main non-metallic constituents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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Abstract
The invention belongs to the technical field of ceramic reinforced metal matrix composite materials, and particularly relates to a SiC reinforced copper matrix composite material and a preparation method thereof. The SiC reinforced copper-based composite material comprises Cu particles and SiC particles, wherein an amorphous glass phase is arranged between the Cu particles and the SiC particles, and the amorphous glass phase is SiO2And Cu2And O eutectic. According to the invention, the amorphous glass phase is introduced between the SiC particles and the Cu particles as an interface transition layer, so that the direct contact between the SiC particles and the Cu particles is avoided, and the performance of the SiC reinforced copper-based composite material is improved.
Description
Technical Field
The invention belongs to the technical field of ceramic reinforced metal matrix composite materials, and particularly relates to a SiC reinforced copper matrix composite material and a preparation method thereof.
Background
Pure copper has advantages of high electrical conductivity, high thermal conductivity, low thermal expansion coefficient, etc., and is widely used in the fields of electronics, thermoelectricity, etc. However, pure copper has poor mechanical properties such as strength and hardness, and thus has limited applications. In practical application, strengthening treatment of pure copper materials is an indispensable link. The addition of a solid particulate reinforcing phase to the copper matrix is an effective strengthening treatment, with SiC particles being a commonly used reinforcing phase. As shown in the Roche's treatise on the Roche's Law of Wangchunhua at Zhengzhou university, SiC-reinforced copper-based composites (SiC/Cu composites) combine the advantages of high electrical and thermal conductivity and processability of metal matrix copper and the performance of reinforced phase SiC, such as high strength, high wear resistance, low density and low expansion coefficient (SiCpStudy of the electrical conductivity characteristics of the/Cu composite).
However, when the SiC particles are used as a reinforcing phase to synthesize the SiC reinforced copper-based composite material, the following problems exist: the wettability between two phases of SiC particles and Cu particles is poor, so that the bonding property between the two phases is poor; the thermal expansion coefficients of the SiC particles and the Cu particles are not matched, and interface thermal stress exists at an interface, so that the formed composite material has poor compactness; the SiC particles and the Cu particles can generate interface reaction under the high-temperature condition to generate a plurality of unstable interface products (Cu)xSiyAnd C), thereby reducing the mechanical properties of the composite.
For improving the interface state between SiC particles and Cu particles, the notice number is CN104294071B discloses a SiC reinforced with a low temperature glass phasepa/Cu composite material, wherein the low-temperature glass phase component in the composite material is SiO2And K2And O. The composite material adopts the low-temperature glass phase as an interface layer, improves the interface state of SiC particles and Cu particles, and enables the bending strength of the composite material to reach about 240MPa, but the bending strength of the composite material still cannot meet the use requirement.
Disclosure of Invention
The invention aims to provide a SiC reinforced copper-based composite material, which effectively improves the bending strength of the SiC reinforced copper-based composite material.
The invention also aims to provide a preparation method of the SiC reinforced copper-based composite material.
In order to achieve the purpose, the invention adopts the technical scheme that:
the SiC reinforced copper-based composite material comprises Cu particles and SiC particles, wherein an amorphous glass phase is arranged between the Cu particles and the SiC particles, and the amorphous glass phase is SiO2And Cu2And O eutectic.
The invention introduces SiO between SiC particles and Cu particles2And Cu2The amorphous glass phase formed by O is used as an interface transition layer, so that direct contact between SiC particles and Cu particles is avoided, the interface bonding strength of the SiC particles and the Cu particles is improved, the compactness and the mechanical property of the SiC reinforced copper-based composite material are improved, and the bending strength of the SiC reinforced copper-based composite material can reach more than 300 MPa.
The thickness of the interface transition layer is controlled by regulating and controlling the amount of the introduced amorphous glass phase, the performance of the SiC reinforced copper-based composite material is further improved, and the obtained SiC reinforced copper-based composite material has a thermosensitive effect. Preferably, the mass of the amorphous glass phase is 3-10% of the total mass of the Cu particles and the SiC particles.
By the reaction of SiO2And Cu2Control of the quality of O to optimize the structure of the amorphous glass phase formed, preferably SiO in the amorphous glass phase2And Cu2The mass ratio of O is 8: 92.
in order to improve the matching degree of SiC particles and Cu particles, the average particle size of the SiC particles is 1-5 mu m, and the average particle size of the Cu particles is 1-2 mu m.
Preferably, the volume ratio of the SiC particles to the Cu particles is 1: 3.
the preparation method of the SiC reinforced copper-based composite material adopts the technical scheme that:
a preparation method of a SiC reinforced copper-based composite material comprises the following steps: mixing SiC composite powder and Cu2Uniformly mixing O powder and Cu powder to obtain mixed powder; then prepressing the mixed powder and then sintering in vacuum to obtain the powder; the SiC composite powder is amorphous SiO2Composite powder wrapping SiC particles.
In the vacuum sintering process, Cu particles in the Cu powder are softened, SiC particles are not softened, the Cu particles generate plastic deformation, and the Cu atoms are necessarily diffused in the plastic deformation process, so that gaps among the SiC particles are filled with the Cu particles, and the density of the composite material is improved. Amorphous SiO2And Cu2And O forms an amorphous glass phase, and the amorphous glass phase is uniformly filled between SiC particles and Cu particles to form an interface transition layer due to viscous flow, so that the densification capability of the composite material is improved. The preparation method of the invention has simple operation and does not introduce other impurities in the preparation process.
And (3) discharging air holes in the mixed powder by pre-pressing, so as to be beneficial to realizing densification, preferably, the pre-pressing is to pre-press the mixed powder for 4-6 min under the pressure of 25-35 MPa, and release the pressure.
Preferably, the vacuum sintering is specifically as follows: after prepressing, preserving heat for 8-12 min at the temperature of 250-350 ℃; and then preserving heat and pressure for 1-2 h at 700-900 ℃ and under the pressure of 25-35 MPa.
The prepressing and the vacuum sintering are both carried out in a vacuum hot-pressing furnace. And vacuumizing the furnace chamber by using a vacuum pump in the pre-pressing and vacuum sintering processes, so that the vacuum degree is basically maintained at about 0.
For improving the uniformity of the mixed powder, SiC composite powder and Cu2And mixing the O powder and the Cu powder uniformly by adopting a wet grinding mode. Preference is given toThe wet milling adopts a ball milling mode, and the ball-to-material ratio during ball milling is 10: 1, the rotating speed does not exceed 120 r/min.
In the preparation method, the SiC composite powder is prepared by the following steps: uniformly mixing silicate ester and a solvent, adjusting the pH to 2-3, then adding SiC, uniformly mixing, and adjusting the pH to 8-9 to obtain gel; and then washing, drying and crushing the gel to obtain the gel.
First using amorphous SiO2The SiC particles are wrapped, so that direct contact between the SiC particles and the Cu particles in the subsequent preparation process is avoided. Preferably, the solvent is ethanol and water, and the volume ratio of the silicate ester to the ethanol to the water is (1-5): (2-7): 100. wherein the silicate is preferably ethyl orthosilicate.
Drawings
FIG. 1 is an XRD pattern of SiC reinforced copper-based composite materials prepared in examples 5 to 9 of the present invention;
FIG. 2 is an SEM photograph of a fracture of the SiC-reinforced copper-based composite material of example 1 of the present invention;
FIG. 3 shows the results of the flexural strength test of SiC reinforced copper-based composites prepared in examples 5 to 24 of the present invention and of SiC reinforced Cu-based composites of comparative examples 1 to 5;
FIG. 4 is a graph showing the temperature-dependent change in electrical resistance of the SiC-reinforced copper-based composite material obtained in example 8 of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples.
First, examples of SiC-reinforced copper-based composite Material
Example 1
The SiC-reinforced copper-based composite material of the present example included Cu particles (average particle diameter of 1 μm) and SiC particles (average particle diameter of 1 μm), the volume ratio of the Cu particles to the SiC particles being 1: 3; an amorphous glass phase is arranged between the Cu particles and the SiC particles, wherein the amorphous glass phase is SiO2And Cu2O (mass ratio of the both is 8: 92), and the mass of the amorphous glass phase is 3% of the total mass of the SiC particles and the Cu particles.
Example 2
The SiC-reinforced copper-based composite material of the present example included Cu particles (average particle diameter of 1 μm) and SiC particles (average particle diameter of 1 μm), the volume ratio of the Cu particles to the SiC particles being 1: 3; an amorphous glass phase is arranged between the Cu particles and the SiC particles, wherein the amorphous glass phase is SiO2And Cu2O (mass ratio of the both is 8: 92), and the mass of the amorphous glass phase is 5% of the total mass of the SiC particles and the Cu particles.
Example 3
The SiC-reinforced copper-based composite material of the present example included Cu particles (average particle diameter of 1 μm) and SiC particles (average particle diameter of 1 μm), the volume ratio of the Cu particles to the SiC particles being 1: 3; an amorphous glass phase is arranged between the Cu particles and the SiC particles, wherein the amorphous glass phase is SiO2And Cu2O (mass ratio of the both is 8: 92), and the mass of the amorphous glass phase is 9% of the total mass of the SiC particles and the Cu particles.
Example 4
The SiC-reinforced copper-based composite material of the present example included Cu particles (average particle diameter of 1 μm) and SiC particles (average particle diameter of 1 μm), the volume ratio of the Cu particles to the SiC particles being 1: 3; an amorphous glass phase is arranged between the Cu particles and the SiC particles, wherein the amorphous glass phase is SiO2And Cu2O (mass ratio of the both is 8: 92), and the mass of the amorphous glass phase is 7% of the total mass of the SiC particles and the Cu particles.
Second, example of the method for producing SiC-reinforced copper-based composite Material
Examples 5 to 24
The preparation methods of the SiC reinforced copper-based composite materials of embodiments 5 to 24 all include the following steps:
(1) pouring 100mL of deionized water into a cleaned and dried 250mL beaker, adding absolute ethyl alcohol and ethyl orthosilicate to form a solution, and adding citric acid to adjust the pH of the solution to 2-3; then 16.05g SiC (average particle size of 1 μm, density of 3.2g/cm) was added, and the beaker was placed in a thermostatic waterbath stirrer with water temperature set at 40 ℃ and heated in a waterbath for 4 hours to hydrolyze the tetraethoxysilane completely to form SiO2Sol to obtain a mixed solution A;
(2) dropwise adding dilute ammonia water (ammonia water: water is 1: 4 (volume ratio), the concentration of the ammonia water is 3.7mol/L) into the mixed solution A by using a rubber head dropper, adjusting the pH to 8-9, and continuously stirring for reaction for 2 hours to obtain SiO2A wrapped SiC composite gel B; washing and filtering the composite gel B, and drying to obtain a block-shaped substance C; grinding the bulk material C by a planetary ball mill to obtain amorphous SiO2Composite powder wrapping SiC;
(3) amorphous SiO2SiC-coated composite powder and Cu2Mixing and ball-milling for 15min, adding 134.82g of Cu powder (with the average particle size of 1 micron and the density of 8.96g/cm) for mixing, adding ethanol, uniformly dispersing by adopting a wet mixing method, ball-milling at a low speed for 1h (the ball-material ratio is 10: 1 and the rotating speed is 120r/min), and then drying in vacuum (drying at the temperature of 60 ℃ for 12h) to obtain mixed powder;
(4) placing 27g of the mixed powder in a mould matched with a vacuum hot-pressing furnace, and then placing the mould in a furnace chamber; vacuumizing, pre-pressing at room temperature under 30MPa for 5min, and releasing pressure; then heating from room temperature to 300 ℃ (the heating rate is 10 ℃/min) and preserving heat for 10 min; and then heating to the sintering temperature from 300 ℃ and pressurizing to 30MPa (the heating rate is 10 ℃/min, the pressure increasing rate is increased to 30MPa within 1 min), then keeping the temperature and the pressure for 1h, cooling to the room temperature along with the furnace, and then releasing the pressure to obtain the ceramic material.
Wherein the absolute ethyl alcohol, tetraethoxysilane, citric acid and Cu adopted in each embodiment2The amount of O and the sintering temperature are specifically shown in Table 1.
TABLE 1 amounts of raw materials used in the examples
In examples 5 to 24, the products obtained by the preparation methods of examples 5 to 9 correspond to the composite material in example 1; examples the products prepared by the preparation methods of examples 6-14 correspond to the composite material in example 2; the product prepared by the preparation method of the embodiment 15-19 corresponds to the composite material in the embodiment 3; the products prepared by the preparation methods of examples 20-24 correspond to the composite material in example 4.
Third, comparative example section
Comparative example 1
The SiC reinforced Cu-based composite of this comparative example was prepared by the following method:
(1) taking 16.05g of SiC (with the average particle size of 1 mu m), putting the SiC into a ball milling tank, then adding 134.82g of Cu powder (with the average particle size of 1 mu m) and adding absolute ethyl alcohol, and uniformly dispersing the mixture by adopting a wet mixing method; after ball milling for 1h at low speed, taking out and vacuum drying to obtain a powder composite material;
(2) taking 27g of powder composite powder, putting the powder composite powder into a matched mould of a vacuum hot-pressing furnace, and putting the powder composite powder into a furnace chamber; vacuumizing, pre-pressing at room temperature under 30MPa for 5min, and releasing pressure; then heating from room temperature to 300 ℃ (the heating rate is 10 ℃/min) and preserving heat for 10 min; and then heating to 700 ℃ from 300 ℃ and pressurizing to 30MPa (the heating rate is 10 ℃/min, the pressure increasing rate is increased to 30MPa within 1 min), then keeping the temperature and the pressure for 1h, cooling to room temperature along with the furnace, and then releasing the pressure to obtain the catalyst.
Comparative examples 2 to 5
The preparation method of the SiC reinforced Cu-based composite material in the comparative examples 2 to 5 is basically the same as that of the comparative example 1, and the difference is only that: in the step (2) in the comparative example 2, the temperature is increased from 300 ℃ to 750 ℃; in the step (2) in the comparative example 3, the temperature is increased from 300 ℃ to 800 ℃; in the comparative example 4, the temperature in the step (2) is increased from 300 ℃ to 850 ℃; in comparative example 5, the temperature in step (2) was raised from 300 ℃ to 900 ℃.
Fifth, test example section
Test example 1
Phase characterization is performed on the SiC reinforced copper-based composite materials of the embodiments 5-24 by using an X-ray diffraction analyzer (XRD), so that phase change of the raw materials and the preparation process thereof and phase composition of the final SiC reinforced copper-based composite material are obtained through analysis, and XRD test results of the SiC reinforced copper-based composite materials of the embodiments 5-9 are shown in figure 1. The XRD test results of the SiC-reinforced copper-based composites of examples 10 to 24 were the same as those of the SiC-reinforced copper-based composites of examples 5 to 9.
As can be seen from FIG. 1, the main crystal phases in the obtained SiC reinforced copper-based composite material were Cu and SiC, and no other diffraction peaks appeared, while it was also shown that no other impurities were introduced during the preparation process. It is shown that the difference of the sintering temperature has no influence on the composition of the SiC reinforced copper-based composite material.
Test example 2
The microscopic morphology of the fracture (fracture obtained when the sample was crushed when three-point bending resistance was tested) of the composite material in example 1 was examined and analyzed using a Scanning Electron Microscope (SEM) model JSM-7001F from Japan Electron (JEOL), as shown in fig. 2. As can be seen from fig. 2, a glass phase exists between the reinforcing phase SiC particles and the Cu particles, and the interface bonding state thereof is improved.
Test example 3
The bending strength (bending strength) of the SiC reinforced copper-based composite materials prepared in examples 5 to 14 and the SiC reinforced Cu-based composite materials in comparative examples 1 to 5, which is the maximum ability of the experimental sample to resist bending without breaking, i.e., the maximum stress of the tensile surface of the sample at the time of breaking under the action of bending stress, was tested in the following specific test manner: the bending strength of the sample is tested by adopting a three-point bending method, and the bending strength is tested by using a WD-P4504 type high-temperature electronic universal testing machine of a Jinnantai instrument in the experiment. According to the national standard YB/T5349-2006 of the metal bending mechanical property testing method, a standard sample strip with the size of 5mm multiplied by 20mm is prepared, the span of an instrument is adjusted to 14.5mm during testing, constant speed loading (the loading rate is 0.5mm/min) is adopted, 3 sample strips are selected for testing the bending strength of a sample under the same experimental condition, and finally the average value of the bending strength is calculated. The test results are shown in fig. 3.
As can be seen from FIG. 3, SiO is introduced into the SiC-reinforced copper-based composite material2And Cu2The bending strength of the composite material is improved after the amorphous Glass Phase (GP) is formed by O. At the same sintering temperature, the improvement range of the bending strength is enhanced along with the increase of the content of the introduced amorphous glass phase, but the bending strength is more than 300 MPa. Moreover, the sintering temperature in the preparation process also has an influence on the bending strength of the composite material, and no non-introduction of the additive is carried outThe bending strength of the composite material gradually increases along with the increase of the sintering temperature during the crystal glass phase; after the amorphous glass phase is introduced, the bending strength of the composite material is increased, then decreased and then increased along with the increase of the sintering temperature. Along with the increase of the sintering temperature, the Cu particles are softened to generate plastic deformation, partial air holes are filled, the compactness of the sample is improved, and the bending strength is improved along with the compactness. When the sintering temperature is 800 ℃, the amorphous glass phase generates a liquid phase, but the fluidity is poor due to temperature limitation, the amorphous glass phase is agglomerated together and cooled along with a furnace, the amorphous glass phase at the moment is equivalent to a brittle phase which is agglomerated between SiC and Cu interfaces in a large quantity, and the bending strength is reduced during bending test. Along with the increase of the sintering temperature, the fluidity of the glass phase is enhanced, the gas holes are uniformly distributed between the SiC interface and the Cu interface while being filled, the density of the sample is improved again, and the bending strength is improved along with the increase of the sintering temperature.
Test example 4
The resistance change performance of the SiC reinforced copper-based composite material prepared in the embodiment 5-24 along with the temperature was tested by using an FT-352 conductor material high-temperature resistivity test system. On the surface of the test results, the resistance of the SiC reinforced copper-based composite materials prepared in examples 5 to 24 showed the same rule with the change of temperature, and the test results of the SiC reinforced copper-based composite material prepared in example 8 are illustrated as an example, and are shown in fig. 4.
As can be seen from fig. 4, the resistance of the SiC-reinforced copper-based composite material gradually increases with an increase in temperature from room temperature to around 450 ℃. The occurrence of PTC effects; at around 450 ℃ to 600 ℃, the resistance is reduced and then sharply increased along with the increase of the temperature, the NTC effect appears firstly, and then the PTC effect appears again, and the resistance sharply increases. When the temperature is between about 600 ℃ and about 750 ℃, the constant resistance phenomenon occurs, and the resistance fluctuates in small amplitude up and down at a constant value along with the increase of the temperature. In conclusion, the SiC reinforced copper-based composite material has a thermal sensitive effect and can be used as a thermistor.
Claims (10)
1. The SiC reinforced copper-based composite material is characterized by comprising Cu particles and SiC particles, wherein the Cu particles and the SiC particles are arranged between the Cu particles and the SiC particlesHas an amorphous glass phase which is SiO2And Cu2And O eutectic.
2. The SiC-reinforced copper-based composite material according to claim 1, wherein the mass of the amorphous glass phase is 3 to 10% of the total mass of the Cu particles and the SiC particles.
3. The SiC-reinforced copper-based composite material according to claim 1, wherein the amorphous glass phase is SiO2And Cu2The mass ratio of O is 8: 92.
4. the SiC-reinforced copper-based composite material according to any one of claims 1 to 3, wherein the SiC particles have an average particle diameter of 1 to 5 μm and the Cu particles have an average particle diameter of 1 to 2 μm.
5. The SiC reinforced copper-based composite material according to any one of claims 1 to 3, wherein the volume ratio of the SiC particles to the Cu particles is 1: 3.
6. a method for producing the SiC-reinforced copper-based composite material according to any one of claims 1 to 5, comprising the steps of: mixing SiC composite powder and Cu2Uniformly mixing O powder and Cu powder to obtain mixed powder; then prepressing the mixed powder and then sintering in vacuum to obtain the powder; the SiC composite powder is amorphous SiO2Composite powder wrapping SiC particles.
7. The preparation method of the SiC reinforced copper-based composite material according to claim 6, wherein the pre-pressing is to pre-press the mixed powder for 4-6 min under the pressure of 25-35 MPa and release the pressure.
8. The method for producing the SiC-reinforced copper-based composite material according to claim 6 or 7, wherein the vacuum sintering is specifically: after prepressing, preserving heat for 8-12 min at the temperature of 250-350 ℃; and then preserving heat and pressure for 1-2 h at 700-900 ℃ and under the pressure of 25-35 MPa.
9. The method for preparing the SiC reinforced copper-based composite material according to claim 6, wherein the SiC composite powder is prepared by the following method: uniformly mixing silicate ester and a solvent, adjusting the pH to 2-3, then adding SiC particles, uniformly mixing, and adjusting the pH to 8-9 to obtain gel; and then washing, drying and crushing the gel to obtain the gel.
10. The method for preparing the SiC reinforced copper-based composite material according to claim 9, wherein the solvent is ethanol and water, and the volume ratio of the silicate ester to the ethanol to the water is (1-5): (2-7): 100.
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| CN113930634A (en) * | 2021-09-22 | 2022-01-14 | 郑州航空工业管理学院 | Cu/SiO2-Cu2O/SiC metal matrix composite material and preparation method thereof |
| CN115582547A (en) * | 2022-10-18 | 2023-01-10 | 郑州航空工业管理学院 | Cu/C/SiC composite material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113930634A (en) * | 2021-09-22 | 2022-01-14 | 郑州航空工业管理学院 | Cu/SiO2-Cu2O/SiC metal matrix composite material and preparation method thereof |
| CN113930634B (en) * | 2021-09-22 | 2022-08-12 | 郑州航空工业管理学院 | Cu/SiO 2 -Cu 2 O/SiC metal matrix composite material and preparation method thereof |
| CN115582547A (en) * | 2022-10-18 | 2023-01-10 | 郑州航空工业管理学院 | Cu/C/SiC composite material and preparation method thereof |
| CN115582547B (en) * | 2022-10-18 | 2024-02-23 | 郑州航空工业管理学院 | Cu/C/SiC composite material and preparation method thereof |
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